Deniz Türkmen, Semra İde, Adil Denizli, Rabel Soomro, Veyis Karakoç, Elif Hilal Şen

Isıya duyarlı poli(N-izopropilakrilamit) temelli kriyojellerin SAXS çalışması

Bu çalışmanın amacı, NIPA’in düşük kritik çözelti sıcaklığı (LCST) civarındaki sıcaklığın değiştirilmesiyle ısıya duyarlı poli(N-izopropilakrilamid-metakriloil-L-histidin), poli(NIPA-MAH) monolitik kriyojellerinin nano yapısındaki değişimleri küçük açı x-ışını saçılması (SAXS) yöntemi ile incelemektir. Poli(NIPA-MAH) kriyojeller, NIPA, MAH fonksiyonel monomeri ve N,N-metilen-bisakrilamit (MBAAm) çapraz bağlayıcısı kullanılarak plastik şırınga içerisinde serbest radikal kriyopolimerizasyonu ile hazırlanmıştır. Polimerizasyon buz banyosunda sıfır derecenin altında N, N, N, N-tetrametilen diamin (TEMED) ve amonyum persulfat (APS) çifti kullanılarak başlatılmıştır. Poli(NIPA-MAH) kriyojelinin LCST değeri 34ºC olarak bulunmuştur. Poli(NIPA-MAH) kriyojelleri 60-100 µm gözenek çapına ve 42.6m2 /g polimer spesifik yüzey alanına sahiptir. Sentezlenen gözenekli kriyojeller geleneksel jellerle karşılaştırıldığında sıcaklık değişimine hızlı tepki vermektedir. Poli(NIPA-MAH) kriyojelinin yığın yapısı ve yüzey morfolojisi taramalı elektron mikroskobu (SEM) kullanılarak belirlenmiştir. SAXS, poli(NIPA-MAH) kriyojelinin sıcaklık değişimiyle gözenek hacmi, duvar kalınlığı ve gözenek şekli gibi nano boyuttaki değişimlerin belirlenmesine imkan vermektedir. 30-40oC sıcaklık aralığında doğal form ve su içerisinde saçılma verileri incelenmiştir. Iki farklı sıcaklıkta (34º C ve 35ºC)gözenek boyutu ve şekli üzerinde kaydedilebilir bir değişikliği gösteren ayrıntılı bir inceleme de gerçekleştirilmiştir.

Thermosensitive poly(N-isopropylacrylamide) based cryogel: A SAXS study

The purpose of this study is to observe the structural changes of the thermosensitive poly(N-isopropylacrylamideN-methacryloyl-L-histidine) poly(NIPA-MAH) monolithic cryogel with changing temperature around lower critical solution temperature (LCST) of NIPA by Small Angle X-Ray Scattering (SAXS). Poly(NIPA-MAH) cryogel was prepared by free radical cryocopolymerization of NIPA with MAH as functional comonomer and N,Nmethylene-bisacrylamide (MBAAm) as crosslinker directly in a plastic syringe. Polymerization initiated by N,N,N,Ntetramethylene diamine (TEMED) and ammonium persulfate (APS) pair at subzero temperature in an ice bath. LCST of poly(NIPA-MAH) cryogel was found to be 34ºC. Poly(NIPA-MAH) cryogel with 60–100 µm in pore diameter have a specific surface area of 42.6 m2/g polymer. This porous cryogel form provides fast temperature response comparing to conventional gels. The surface morphology and bulk structure of poly(NIPA-MAH) cryogel revealed with scanning electron microscopy (SEM). SAXS allowed the determination of nanoalteration of poly(NIPA-MAH) cryogel such as pore volume, wall thickness and pore shape with changing temperature. Scattering data were analysed both native form and in water at temperature range of 300C-400C. At two different temperatures 34º Cand 35ºC a detailed investigation on shape of pores and pore size; which indicating a recordable change, were also carried out.

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